Agglomeration process including a heating step for making a free-flowing granulate

Abstract

A free-flowing granulate of a powder-form or fine-grained component and a liquid component; the granulate containing at least 20% by weight of the liquid component, is prepared by moving the powder-form or fine-grained component in a mixer-granulator, adding the liquid component while mixing until a moist granulate having a particle size of at most 1.5 mm is obtained, subsequently coarsening the granulate thus obtained with an increase in temperature to a particle size of from 0.4 to 4 mm and optionally coating this coarse granulate with another powder-form and/or fine-grained component at 60 DEG to 90 DEG C. The optionally coated granulate is converted by lowering the treatment temperature into a dry-looking, free-flowing, coarse-grained product, which if desired, may be coated with another powder-form and/or fine-grained material. Despite the high percentage of a liquid component, the granulate thus obtained appears as a dry granulate and is free-flowing.

What is claimed is: 
     
       1. A process for the production of a free-flowing granulate consisting of a powder-form or fine-grained dry component and a liquid component, wherein the granulate contains from about 20% to 30% by weight of the liquid component, comprising the steps of: (a) imparting movement to a first dry powder-form or fine-grained component, having a particle size up to about 1 mm; wherein said first dry component is a detergent, washing aid, or fabric treatment preparation;   (b) adding a liquid component to the moving first dry component; wherein said liquid component is a detergent, washing aid, or fabric treatment preparation;   (c) mixing the first dry component and the liquid until a substantially non-free-flowable moist granulate having a particle size of at most 1.5 mm is obtained;   (d) heating the moist granulate from step (c) to a temperature of about 60° to 90° C. to aggomerate the moist granulate and form a coarse-grained moist, substantially non-free-flowable granulate having a particle size of from 0.4 mm to 4.0 mm;   (e) optionally mixing the moist granulate from step (d) with a first material comprising a second powder-form or fine-grained dry component or a mixture of the second dry component and a liquid component at 60° to 90° C., m to obtain a granulate coated with said second dry component or mixture thereof;   (f) lowering the temperature by from about 5° to 10° C. with continuous movement to obtain a dry-looking, free-flowing coarse-grained granulate product wherein at least 50% of the product has a particle size of from about 0.4 to 4 mm; and   (g) optionally subjecting at least part of the granulate product from step (f) to steps (e) and (f).   
     
     
       2. A process in accordance with claim 1, wherein step (a) is carried out in a mixer-granulator. 
     
     
       3. A process in accordance with claim 1, wherein step (d) is carried out in a grain-coarsening unit. 
     
     
       4. A process in accordance with claim 1, wherein process steps (a) through (c) are carried out in a mixer-granulator in which mixing is effected by moving mixing elements. 
     
     
       5. A process in accordance with claim 1, wherein process steps (d) through (g) are carried out in fluidized-bed. 
     
     
       6. The process of claim 1, wherein the first dry component is highly disperse silica, a filler, a disintegrating agent, a bleach activator, a per compound, a fabric softener, a quaternary ammonium compound containing one or two long residues, a soluble or insoluble builder salt, a clay, a heavy metal complexing agent, a discoloration inhibitor, redeposition inhibitor, an enzyme, an optical brightener, a foam regulator, a dye, a powder-form washing-active substance, or a mixture thereof; and said liquid component is a liquid or liquefied or dissolved or dispersed washing-active substance, a foam regulator, a builder salt, a heavy metal complexing agent, a perfume, water, an organic solvent, a wax, or an oil. 
     
     
       7. A process in accordance with claim 6, wherein the liquid component is an alcohol ethoxylate. 
     
     
       8. A process in accordance with claim 1, wherein process step (e) is carried out with a mixture or fine-grained granulate of sodium perborate and alcohol ethoxylate. 
     
     
       9. A process in accordance with claim 8, wherein the alcohol ethoxylate is a C 14  -C 15  oxoalcohol with 7 moles of ethylene oxide. 
     
     
       10. A process in accordance with claim 1, wherein process step (e) is carried out by first mixing the moist granulate from step (d) with the first material and then with a second material, the first material being selected in such a way that it is compatible both with the product of process steps (a) to (d) and with the second material. 
     
     
       11. The process of claim 1, including step (e). 
     
     
       12. The process of claim 1, wherein the first dry component is highly dispersed precipitated silica, sodium aluminum silicate, sodium perborate, tetraacetylethylene diamine, or a C 8  -C 20  -alkyl trimethylammonium salt or a mixture thereof; and said liquid component is a non-ionic surfactant, an adduct of from 1 to 6 moles ethylene oxide with one mole of a primary fatty amine containing a C 10  -C 16  -alkyl or alkenyl group, the sodium salt of β-aminoalkyl- or β-aminoalkenylpropionic acid, silicone oil, or a solution of a heavy metal complexing agent. 
     
     
       13. A process for the production of a free-flowing granulate consisting of a powder-form or fine-grained dry component and a liquid component, wherein the granulate contains at least 20% by weight of the liquid component, comprising the steps of: (a) imparting circular movement to a first dry powder-form or fine-grained component, having a particle size up to about 1 mm; said powder-form or fine-grained component comprising: from about 5 to about 55 parts by weight of highly disperse precipitated silica or sodium aluminosilicate;   from about 3 to about 20 parts by weight of tetradecyltrimethylammonium salt;   from about 1 to about 5 parts by weight of a premix of about 4 parts by weight of polydimethylsiloxane and about 6 parts by weight of highly disperse precipitated silica; and, optionally, from about 10 to about 40 parts by weight of tetraacetyl ethylene diamine;     (b) spraying successively or simultaneously onto the moving mixture a liquid component comprising: from about 15 to 45 parts by weight alcohol ethoxylate; and   from about 1 to 10 parts by weight of an about 10 to 40% by weight aqueous solution of a heavy metal complexing agent;     (c) mixing the first dry component and the liquid until a substantially non-free-flowable moist granulate having a particle size of at most 1.5 mm is obtained;   (d) heating the moist granulate from step (c) with hot air in a fluidized bed to about 60°-90° C. to agglomerate the first dry component particles and form a coarse-grained moist, substantially non-free-flowable granulate having a particle size of from 0.4 mm to 4.0 mm;   (e) optionally mixing the moist granulate from step (d) with a first material comprising a second powder-form or fine-grained dry component or a mixture of the second dry component and a liquid component at 60° to 90° C., to obtain a granulate coated with said second dry component or mixture thereof;   (f) lowering the temperature in the fluidized bed by from about 5° to 10° C. with continuous movement to obtain a dry-looking, free-flowing coarse-grained granulate product wherein at least 50% of the product has a particle size of from about 0.4 to 4 mm; and   (g) optionally subjecting at least part of the granulate product from step (f) to steps (e) and (f).